1'-(phenylmethyl)-[1,4'-bipiperidine]-4'-carbonitrile

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2017-03-13 to 2017-05-12

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2017

Report date:

2017

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

Test guideline 3

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

1'-(phenylmethyl)-[1,4'-bipiperidine]-4'-carbonitrile

EC Number:

282-544-0

EC Name:

1'-(phenylmethyl)-[1,4'-bipiperidine]-4'-carbonitrile

Cas Number:

84254-97-7

Molecular formula:

C18H25N3

IUPAC Name:

1'-benzyl-[1,4'-bipiperidine]-4'-carbonitrile

Test material form:

solid: particulate/powder

Specific details on test material used for the study:

- Batch n°: I15IB3393
- Analytical purity: 99.93%
- Expiration date: 2017-10-25
- Storage condition: at room temperature

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

106.1 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Remarks:

A dark yellow to orange/brown molten residue remained after the preliminary and main test, indicating reaction and/or decomposition.

Decomp. temp.:

> 150 °C

Any other information on results incl. tables

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly at 225°C. At 320°C the sample weight has decreased by 25%. After the experiment, an orange/brown molten residue remained in the sample container (original colour: beige). The change of the colour indicated reaction and/or decomposition of the test item.

Main tests

In order to determine the melting more precisely, the DSC curve with a heating rate of 20°C/min was obtained and showed an endothermic peak between 75°C and 125°C. The extrapolated onset temperature of the peak was 105.956°C. The effect was most likely obtained due to melting. A second endothermic peak was observed between 150°C and 320°C due to reaction and/or decomposition of the test item. After the experiment, a dark yellow molten residue remained. To investigate the melting peak between 75°C and 125°C, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 106.149°C. The melting temperature of T000745 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 106.1°C (379.2K).

Applicant's summary and conclusion

Conclusions:

The melting temperature of JNJ-1594983-AAA (T000745) was determined at 106.1°C (379.2K) by using DSC.